Daunorubicin (DRB) and cytarabine (CYT) are medications used to treat cancer agents used in chemotherapy, and a standardized and reliable technique for estimating their concentration in bulk tablet form was established utilizing RP-HPLC. Mobile phase (KH2PO4: Acetonitrile of 50:50) was passed through an STD AGILENT 150 x 4.6 mm,5 columns at a rate of 1.0 ml/min. The retention time of DRB equaled 2.255 minutes, whereas that of CYT equaled 2.963 minutes. The relative standard deviations (RSDs) of DRB and CYT being 0.9 and 0.6, correspondingly, the percentages of drugs recovered were 100.15 and 100.42, correspondingly. Regression models for both DRB and CYT yielded LOQ and LOD values of 0.21 and 0.64, and 0.45 and 1.35, correspondingly. Overall, the % yield was 100% for both CYT and DRB. The regression equation for DRB is y = 37361.x + 4337, but that for CYT is y = 41833.x + 24623.